Manufacture of synthetic resins



Patented June 9, 1936 UNITED STATES PATENT OFFICE MANUFACTURE OF SYNTHETIC RESINS Henry G. Berger, Woodbury, N. J., assignor to Socony-Vacuum Oil Company, Incorporated, New York, N. Y., a corporation ofNew York No Drawing. Application January 26,1935,

Serial No. 3.649

4 Claims. (01. 260-2) This invention relates to the manufacture of synthetic resins by the use of petrolatum as the basic, material. The object of the invention is, primarily, the production of hard, infusible and 5 insoluble resins suitable for molding under combiried heat and pressure, and, secondarily, to provide for the economical utilization of the petrolatum which is produced, in excess of other rereaction mixture a volatile chlorinated hydrocar-' bon, such as carbon tetrachloride, which serves not only as a solvent for the petrolatum, but also as a conveyor for the chlorine which promotes the condensing reaction and also enters into the flnal composition of the resin. I have discovered that when working in this manner the product is a hard resin, of superior character for use in molding compositions, which is insoluble in all ordinary solvents and will become plastic when heated to about 106 C., but will not melt at any temperature below that at which it decomposes. Furthermore, the production of the, resin in this manner is simplified by the fact that, if the chlorinated volatile hydrocarbon has been used in, or in excess of, equivalent proportion with the petrolatum, the decomposition 'of the reaction complex by the addition of water causes the resin to separate in solid form, needing only to be ground and washed to prepare it in suiilciently 40 pure condition for use.

In place of carbon tetrachloride, I have found that chlorinated naphtha, chlorinated petroleum propane or penta-chlor butane may be used with substantially the same efiect. Anhydrous aluminum chloride is the catalyst most economically available for use in my process, but the other active metal halides well known to produce similar condensing reactions may be used if preferred- As an example of my process, 100 parts, by

weight, of petrolatum may be heated with 100 parts of anhydrous aluminum chloride, to a temperature of C., and parts of carbon tetra-' chloride added slowly. The mixture is heated until the evolution of gas ceases. and water or 55 ,dilute hydrochloric acid is then added, and the mixture is stirred until it separates into solid resin and'a water solution. The wet resin may then be ground, washed with water and dried.

' 'Iheyieldofresinis-aboutflparts.

In the example just given the petrolatum and the,carbon tetrachloride are in approximately molecular proportion andare substantially all consumed. It is usually more convenient to use the carbon tetrachloride in considerable excess, I as, for example, 15 or 16-parts to one part of petrolatum. In this case the excess of the tetrachloride may be recovered by decantation, prior to the addition of water to the reaction complex.

I have not determined the molecular proportions l0 for the other volatile chlorinated hydrocarbons,

but either of them may be used in-excess, as in the case of the carbon tetrachloride, and the'excess' recovered in the same way. In each case the yield of resin will be based on the quantity of 16 petrolatum and will be approximately the same as in the given example, and the resin will have the same characteristics.

The resins-produced by this method are brittle, when used alone, having a conchoidal fracture 20 and a dark brown color, and they contain substantial quantities of chlorine, of the order of 3% to 13% or more. v When mixed with wood flour or other inert fillers they constitute excellent molding compositions, for forming under 25 combined. heat and pressure.

This application is a continuation, in part,- of my application filed July 3, 1934. Serial No. 733,605.

I claim as my invention: 30

1. The method of manufacturing a hard, heatplastic insoluble resin, which comprises the steps of reacting petrolatum with volatile chlorinated hydrocarbon material selected from the class consisting of carbon tetrachloride, chlorinated 35'- petrolatum is substantially all condensed, and 45 decomposing the reaction complex and washing the resultant resin with water.

3. The method set forth in claim 1, as practiced with the said volatile chlorinated hydrocarbon material insubstantial excess of equivalent proportion with the petrolatum.

, 4. The method of manufacturing a hard, heatplastic resin, which comprises the steps of reacting petrolatum with a chlorinated volatile hydrocarbon in the presence of an active metal halide until the petrolatum is substantially all condensed. and decomposing the reaction complex and washing the resultant resin with water.

HENRY G. BERGER. 

